Reaktion #67488

ord-7e785c72c2ab42aea1a644c10c35ba43

Reaktionsgleichung

CN[C@@H](CCC(=O)O)C(=O)O
N-methylglutamic acid
O=S(=O)(O)O
sulfuric acid
→
CN[C@@H](CCC(=O)O)C(=O)O.O=S(=O)(O)O
N-methylglutamic acid sulfate
Ausbeute 97.8%

Edukte

CN[C@@H](CCC(=O)O)C(=O)O
N-methylglutamic acid
O=S(=O)(O)O
sulfuric acid

Reagenzien

Keine

Lösungsmittel

O
water

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigefor 30 minutes
  2. 2
    workup.STIRRINGunder stirring
  3. 3
    workup.STIRRINGstirred for additional 2 hours
  4. 4
    SonstigeAfter the reaction
  5. 5
    Einengenthe reaction solution was concentrated
  6. 6
    Sonstigeazeotroped with toluene
  7. 7
    Sonstigeto further remove the water
  8. 8
    Sonstigedried under vacuum

Vorschrift

10.65 g of N-methylglutamic acid was placed in a 250 ml round-bottom flask, and 100 ml of water was added to the flask and stirred by using a magnetic stirrer for 30 minutes. Then, 6.38 g of concentrated sulfuric acid (concentration: 98%) was slowly dropped into the flask under stirring, and stirred for additional 2 hours after dropping. After the reaction, the reaction solution was concentrated, azeotroped with toluene to further remove the water and dried under vacuum to obtain 16.5 g of N-methylglutamic acid sulfate as yellow oil (Yield: 97.7%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524895B2uspto-grants-2013_09